CN114989325A - Ultrasonic extraction process for reducing viscosity of tamarind xyloglucan - Google Patents
Ultrasonic extraction process for reducing viscosity of tamarind xyloglucan Download PDFInfo
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- CN114989325A CN114989325A CN202210647229.9A CN202210647229A CN114989325A CN 114989325 A CN114989325 A CN 114989325A CN 202210647229 A CN202210647229 A CN 202210647229A CN 114989325 A CN114989325 A CN 114989325A
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
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Abstract
The invention discloses an ultrasonic extraction process for reducing viscosity of tamarind xyloglucan, which comprises the following steps: (1) peeling tamarind seeds, crushing, degreasing, deproteinizing to obtain degreased and deproteinized tamarind kernel powder; (2) mixing degreased and deproteinized tamarind kernel powder with water according to a material-liquid ratio of 1g: 30-35 mL, carrying out ultrasonic treatment at 65-75 ℃ for 85-95 min at 170-180W, standing, centrifuging, mixing supernate with an ethanol solution, standing at 3-5 ℃ for 1.5-2.5 h, filtering to obtain a white precipitate, washing, re-dissolving in water, and carrying out vacuum freeze drying to obtain tamarind xyloglucan. The invention adopts an ultrasonic extraction process, has simple and convenient operation, can reduce the molecular weight of polysaccharide products so as to reduce the viscosity of the polysaccharide products, has better physiological activity, can improve the yield of the polysaccharide, and does not influence the primary structure of the polysaccharide.
Description
Technical Field
The invention belongs to the technical field of plant polysaccharide extraction, and particularly relates to an ultrasonic extraction process for reducing viscosity of tamarind xyloglucan.
Background
Tamarind seed (Tamarindus indica L.) belongs to dicotyledonous plants, and the seed is a byproduct produced in tamarind pulp processing and consists of 30% of a fruit shell and 70% of a kernel. The tamarind kernel contains a large amount of polysaccharides, and the content of polysaccharides is 80.66% by calculation using the differential method. Tamarind seed polysaccharides belong to the xyloglucan family.
Xyloglucan (Xyloglucan, XyG), a class of plant cell wall polysaccharides, is present in essentially all plants, differing in content. In dicotyledonous plants, especially tamarind nucleolus, the content of XyG is high, so tamarind nucleolus is one of the most abundant sources of XyG, and many researches are made on it.
Tamarind XyG is a polysaccharide substance present in tamarind kernels, can be dissolved in water to form a viscous aqueous solution, and has physiological activities of reducing blood sugar, blood fat, inflammation and the like. Usually, the yield of water extraction XyG (WE-XyG) is low and takes long time, and the larger molecular weight of the water extraction XyG results in weaker diffusion capability in biological tissues; the higher viscosity is not favorable for uniformly mixing with other substances, thereby preventing the application of the product in the fields of food, medicines and the like. Researchers have used acids or bases to extract tamarind XyG to increase its yield. However, the aqueous solution of the tamarind kernel powder is viscous, so the method of adding acid or alkali is not easy to operate, has larger error and low repeatability. For high viscosity XyG, researchers often use glycosidase treatments to reduce their viscosity for application. However, this method increases the cost and the operation steps, which is not suitable for practical use. Therefore, it is necessary to find a suitable extraction method to effectively increase the yield of tamarind XyG and to reduce its molecular weight and viscosity to increase its economic benefits.
Disclosure of Invention
Aiming at the prior art, the invention provides an ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan, so as to reduce the problems of high viscosity and large operation difficulty of the existing extraction process.
In order to achieve the purpose, the invention adopts the technical scheme that: the ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan comprises the following steps:
(1) peeling tamarind seeds, crushing, degreasing, deproteinizing to obtain degreased and deproteinized tamarind kernel powder;
(2) mixing degreased and deproteinized tamarind kernel powder with water according to a material-liquid ratio of 1g: 30-35 mL, carrying out ultrasonic treatment at 65-75 ℃ for 85-95 min at 170-180W, standing, centrifuging, mixing supernate with an ethanol solution, standing at 3-5 ℃ for 1.5-2.5 h, filtering to obtain a white precipitate, washing, redissolving in water, and carrying out vacuum freeze drying to obtain tamarind xyloglucan.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, peeling comprises the following steps: washing tamarind seeds, soaking in warm water at 80 ℃ for 3-5 h, drying at 70-90 ℃ for 5-7 h, and removing seed coats.
Further, the pulverization comprises the following steps: pulverizing peeled semen Tamarindi Indicae, and sieving with 40 mesh sieve.
Further, the degreasing comprises the following steps: mixing the crushed tamarind seeds with n-hexane, carrying out degreasing treatment at 65-75 ℃ for 3-5 h, removing the upper layer liquid, and standing at room temperature until the n-hexane is completely volatilized.
Further, deproteinization comprises the steps of: mixing the degreased tamarind seeds with water according to a material-liquid ratio of 1g to 9-11 mL, adjusting the pH value to 9-10 by using NaOH, stirring for 25-35 min, centrifuging at 3-5 ℃ and 4000-6000 r/min for 10-20 min, removing supernatant, mixing with water according to a material-liquid ratio of 1g to 9-11 mL, adjusting the pH value to 6.5-7.0 by using 0.8-1.2 moL/L HCL solution, and drying the precipitate.
Further, the centrifugation temperature is 15-25 ℃, the centrifugation speed is 5000-7000 r/min, and the centrifugation time is 15-25 min.
Further, the concentration of the ethanol solution is 94-98 wt%, and the volume ratio of the ethanol solution to the supernatant is 1: 2.
Further, washing is sequentially carried out by using 94-98 wt% of ethanol and absolute ethanol.
Furthermore, the freezing temperature is-70 to-90 ℃.
The invention has the beneficial effects that:
1. the invention increases the movement frequency and speed of substance molecules through ultrasonic waves, enhances the penetrating power of an extraction medium, enables the extraction medium to quickly and effectively contact with a target component, and accelerates the dissolution of the target component.
2. The invention adopts an ultrasonic extraction process, has simple and convenient operation, can reduce the molecular weight of polysaccharide products so as to reduce the viscosity of the polysaccharide products, has better physiological activity, can improve the yield of the polysaccharide, and does not influence the primary structure of the polysaccharide.
Drawings
FIG. 1 is an FTIR spectrum of an ultrasonic extraction of xyloglucan (UAE-XYG) and an aqueous extraction of xyloglucan (WE-XYG).
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention.
Example 1
An ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan comprises the following steps:
(1) cleaning tamarind seed, soaking in 80 deg.C warm water for 4 hr, oven drying at 80 deg.C for 6 hr, removing seed coat, pulverizing, and sieving with 40 mesh sieve to obtain pulverized tamarind seed;
(2) mixing the crushed tamarind seeds with n-hexane, carrying out degreasing treatment at 69 ℃ for 4h, removing upper-layer liquid, and standing at room temperature until the n-hexane is completely volatilized to obtain degreased tamarind seeds;
(3) mixing the degreased tamarind seeds with water according to a feed-liquid ratio of 1g:10mL, adjusting the pH value to 9.5 by using NaOH, stirring for 30min, centrifuging at 4 ℃ at 5000r/min for 15min, removing supernatant, mixing with water according to a feed-liquid ratio of 1g:10mL, adjusting the pH value to 6.8 by using 1moL/L HCL solution, and drying the precipitate to obtain deproteinized tamarind kernel powder;
(4) mixing deproteinized tamarind kernel powder with water according to a feed-liquid ratio of 1g:33mL, performing ultrasonic treatment at 71 ℃ and 175W for 91min, standing for 24h, centrifuging at 20 ℃ and 6000r/min for 20min, mixing supernate with 96 wt% ethanol solution according to a volume ratio of 1:2, standing for 2h at 4 ℃, filtering to obtain white precipitate, sequentially washing with 96 wt% ethanol and absolute ethanol, redissolving in water, and performing vacuum freeze drying at-808 ℃ to obtain tamarind xyloglucan.
Example 2
An ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan comprises the following steps:
(1) cleaning tamarind seed, soaking in 80 deg.C warm water for 3 hr, oven drying at 70 deg.C for 7 hr, removing seed coat, pulverizing, and sieving with 40 mesh sieve to obtain pulverized tamarind seed;
(2) mixing the crushed tamarind seeds with n-hexane, carrying out degreasing treatment at 65 ℃ for 5h, removing upper-layer liquid, and standing at room temperature until the n-hexane is completely volatilized to obtain degreased tamarind seeds;
(3) mixing the degreased tamarind seeds with water according to a feed-liquid ratio of 1g:9mL, adjusting the pH value to 9 by using NaOH, stirring for 25min, centrifuging at 3 ℃ for 20min at 4000r/min, removing supernatant, mixing with water according to a feed-liquid ratio of 1g:9mL, adjusting the pH value to 6.5 by using 0.8moL/L HCL solution, and drying the precipitate to obtain deproteinized tamarind kernel powder;
(4) mixing deproteinized fructus Tamarindi Indicae kernel powder with water at a material-liquid ratio of 1g:30mL, performing ultrasonic treatment at 65 deg.C and 170W for 95min, standing for 24h, centrifuging at 15 deg.C and 5000r/min for 25min, mixing the supernatant with 94 wt% ethanol solution at a volume ratio of 1:2, standing at 3 deg.C for 1.5h, filtering to obtain white precipitate, sequentially washing with 94 wt% ethanol and anhydrous ethanol, redissolving in water, and vacuum freeze-drying at-70 deg.C to obtain fructus Tamarindi Indicae xyloglucan.
Example 3
An ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan comprises the following steps:
(1) cleaning tamarind seed, soaking in 80 deg.C warm water for 5 hr, oven drying at 90 deg.C for 5 hr, removing seed coat, pulverizing, and sieving with 40 mesh sieve to obtain pulverized tamarind seed;
(2) mixing the pulverized tamarind seeds with n-hexane, degreasing at 75 deg.C for 3h, removing the upper liquid, and standing at room temperature until n-hexane is completely volatilized to obtain degreased tamarind seeds;
(3) mixing the degreased tamarind seeds with water according to a feed-liquid ratio of 1g:11mL, adjusting the pH value to 10 by using NaOH, stirring for 35min, centrifuging at 5 ℃ at 6000r/min for 10min, removing supernatant, mixing with water according to a feed-liquid ratio of 1g:11mL, adjusting the pH value to 7.0 by using 1.2moL/L HCL solution, and drying the precipitate to obtain deproteinized tamarind kernel powder;
(4) mixing deproteinized fructus Tamarindi Indicae kernel powder with water at a ratio of 1g:35mL, performing ultrasonic treatment at 75 deg.C and 180W for 85min, standing for 24h, centrifuging at 25 deg.C and 7000r/min for 15min, mixing the supernatant with 98 wt% ethanol solution at a volume ratio of 1:2, standing at 5 deg.C for 2.5h, filtering to obtain white precipitate, sequentially washing with 98 wt% ethanol and anhydrous ethanol, redissolving in water, and vacuum freeze drying at-90 deg.C to obtain fructus Tamarindi Indicae xyloglucan.
Comparative example 1
The ultrasonic power in step (4) in example 1 was changed to 200W.
Comparative example 2
The ultrasonic temperature in step (4) in example 1 was changed to 60 ℃.
Comparative example 3
The sonication time in step (4) in example 1 was changed to 100 min.
Comparative example 4
The feed-liquid ratio of the tamarind kernel powder to water in the step (4) in the example 1 is changed to 1g:40 mL.
Comparative example 5
The sonication in step (4) of example 1 was changed to a water bath treatment (WE-XYG).
The following measurements of the yield and viscosity of tamarind xyloglucan in the examples and comparative examples are shown in table 1.
TABLE 1 yield and viscosity of tamarind xyloglucan
Fourier infrared spectroscopy (FTIR) analysis of tamarind xyloglucan of the invention was performed as follows:
120mg of KBr crystals were weighed out accurately, ground in a small mortar until a fine powder was formed, and tableted. Reference background spectra were collected by pressing with KBr without sample and scanning infrared spectra on an infrared spectrometer. Mixing 120mg KBr crystal and 2mg tamarind XYG sample, grinding, tabletting, and scanning infrared spectrum (500-4000 cm) -1 )。
FTIR can determine which functional groups or chemical bonds are present or altered in the sample. FIG. 1 shows the infrared absorption spectra of an ultrasonic extraction of xyloglucan (UAE-XYG) and an aqueous extraction of xyloglucan (WE-XYG). The main peaks of the infrared spectra of the ultrasonic extraction of xyloglucan (UAE-XYG) and the water extraction of xyloglucan (WE-XYG) are basically the same. The UAE-XYG and WE-XYG samples were at 3418.73cm -1 A broad band appears due to the O-H stretching vibration of the dextran backbone. The sugar chain skeleton of XyG has three characteristic absorption peaks: CH (CH) 2 Bending, C-O bond elongation and C-C bond vibration. Due to CH 2 Bending at 1375.99cm -1 There is a sharp front at 1315.40cm -1 A soft peak is formed; due to the extension of the C-O bond of the XyG ring, at 1040.83cm -1 A strong peak was observed; at 1416.29cm -1 The peak at (a) is caused by the C-C bond vibration. The result shows that the polysaccharide extracted from tamarind kernel is XyG, and the extraction method adopted by the invention has little influence on the functional groups or chemical bonds of XyG.
The results of the tamarind xyloglucan molecular weight distribution measurement of the present invention are shown in table 2 below.
TABLE 2 monosaccharide composition and molecular weight of XYG
| Sample (I) | Ultrasonic extraction of xyloglucan (UAE-XYG) |
| Arabinose (Ara) | 0.174 |
| Glucose (Glu) | 7.832 |
| Galactose (Gal) | 2.029 |
| Xylose (Xyl) | 3.573 |
| Galacturonic acid | 0.045 |
| Glucuronic acid | 0.041 |
| Glu:Xyl:Gal | 3.86:1.76:1 |
| Mw(g/mol) | 1.64×106 |
| PDI(Mw/Mn) | 1.10 |
In the application of tamarind xyloglucan, its properties are often influenced by other substances. Salt and sucrose are two substances often ingested by humans and may have an effect on the apparent viscosity of XyG and thus on XyG application. The apparent viscosities of XyG obtained by the two extraction methods were measured for NaCl solutions and sucrose solutions of different concentrations, and the results are shown in tables 3 and 4.
TABLE 3 n and K for XyGs solutions at different NaCl concentrations
TABLE 4 n and K for XyGs solutions at different sucrose concentrations
As is clear from tables 3 and 4, the apparent viscosity of UAE-XYG was always lower than that of WE-XYG at the same NaCl concentration and sucrose concentration.
While the present invention has been described in detail with reference to the embodiments, it should not be construed as limited to the scope of the patent. Various modifications and changes may be made by those skilled in the art without inventive work within the scope of the appended claims.
Claims (9)
1. An ultrasonic extraction process for reducing the viscosity of tamarind xyloglucan is characterized by comprising the following steps:
(1) peeling tamarind seeds, crushing, degreasing, deproteinizing to obtain degreased and deproteinized tamarind kernel powder;
(2) mixing degreased and deproteinized tamarind kernel powder with water according to a material-liquid ratio of 1g: 30-35 mL, carrying out ultrasonic treatment at 65-75 ℃ for 85-95 min at 170-180W, standing, centrifuging, mixing supernate with an ethanol solution, standing at 3-5 ℃ for 1.5-2.5 h, filtering to obtain a white precipitate, washing, re-dissolving in water, and carrying out vacuum freeze drying to obtain tamarind xyloglucan.
2. The extraction process according to claim 1, characterized in that said peeling comprises the following steps: washing tamarind seeds, soaking in warm water at 80 ℃ for 3-5 h, drying at 70-90 ℃ for 5-7 h, and removing seed coats.
3. The extraction process according to claim 1, characterized in that said pulverization comprises the following steps: pulverizing peeled fructus Tamarindi Indicae seed, and sieving with 40 mesh sieve.
4. The extraction process according to claim 1, characterized in that said degreasing comprises the following steps: mixing the crushed tamarind seeds with n-hexane, carrying out degreasing treatment at 65-75 ℃ for 3-5 h, removing upper liquid, and standing at room temperature until the n-hexane is completely volatilized.
5. The extraction process according to claim 1, characterized in that said deproteinization comprises the following steps: mixing the degreased tamarind seeds with water according to a material-liquid ratio of 1g to 9-11 mL, adjusting the pH value to 9-10 by using NaOH, stirring for 25-35 min, centrifuging at 3-5 ℃ and 4000-6000 r/min for 10-20 min, removing supernatant, mixing with water according to a material-liquid ratio of 1g to 9-11 mL, adjusting the pH value to 6.5-7.0 by using 0.8-1.2 moL/L HCL solution, and drying the precipitate.
6. The extraction process according to claim 1, characterized in that: the centrifugation temperature is 15-25 ℃, the centrifugation speed is 5000-7000 r/min, and the centrifugation time is 15-25 min.
7. The extraction process according to claim 1, characterized in that: the concentration of the ethanol solution is 94-98 wt%, and the volume ratio of the ethanol solution to the supernatant is 1: 2.
8. The extraction process according to claim 1, characterized in that: and the washing is sequentially carried out by using 94-98 wt% of ethanol and absolute ethanol.
9. The extraction process according to claim 1, characterized in that: the freezing temperature is-70 to-90 ℃.
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| CN114181329A (en) * | 2021-12-27 | 2022-03-15 | 青岛琛蓝海洋生物工程有限公司 | Method for extracting xyloglucan in tamarind seeds |
| CN114507295A (en) * | 2021-12-22 | 2022-05-17 | 云南猫哆哩集团食品有限责任公司 | Preparation method of tamarind seed polysaccharide glue solution |
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| JP2012012328A (en) * | 2010-06-30 | 2012-01-19 | Dsp Gokyo Food & Chemical Co Ltd | Xyloglucan-cation complex and stabilized composition containing the same |
| US20130095209A1 (en) * | 2011-10-12 | 2013-04-18 | Ocean Spray Cranberries, Inc. | Xyloglucan extraction process |
| CN108586633A (en) * | 2018-02-08 | 2018-09-28 | 绿麒（厦门）海洋生物科技有限公司 | A kind of quickly water suction is high to be swollen tamarind gum and preparation method thereof |
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| NIPAT LIMSANGOUAN等: "High pressure processing of tamarind (Tamarindus indica) seed for xyloglucan extraction", 《FOOD SCIENCE & TECHNOLOGY》 * |
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